CN219290992U - Gas purification device and glove box - Google Patents
Gas purification device and glove box Download PDFInfo
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- CN219290992U CN219290992U CN202223513797.4U CN202223513797U CN219290992U CN 219290992 U CN219290992 U CN 219290992U CN 202223513797 U CN202223513797 U CN 202223513797U CN 219290992 U CN219290992 U CN 219290992U
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- 238000000746 purification Methods 0.000 title claims abstract description 29
- 238000001179 sorption measurement Methods 0.000 claims abstract description 204
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000001301 oxygen Substances 0.000 claims abstract description 113
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 113
- 239000000463 material Substances 0.000 claims abstract description 84
- 239000007789 gas Substances 0.000 claims abstract description 45
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 230000008929 regeneration Effects 0.000 claims abstract description 30
- 238000011069 regeneration method Methods 0.000 claims abstract description 30
- 239000011261 inert gas Substances 0.000 claims abstract description 25
- 238000011049 filling Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 7
- 230000001172 regenerating effect Effects 0.000 claims description 7
- 238000005485 electric heating Methods 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 238000010926 purge Methods 0.000 abstract description 9
- 230000007246 mechanism Effects 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 54
- 229910052757 nitrogen Inorganic materials 0.000 description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000002808 molecular sieve Substances 0.000 description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 11
- 239000003463 adsorbent Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 229910052802 copper Inorganic materials 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 239000011358 absorbing material Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000007664 blowing Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 239000003446 ligand Substances 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 4
- 239000013067 intermediate product Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 239000005751 Copper oxide Substances 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229940011182 cobalt acetate Drugs 0.000 description 3
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 3
- 229910000431 copper oxide Inorganic materials 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- BSKHPKMHTQYZBB-UHFFFAOYSA-N 2-methylpyridine Chemical compound CC1=CC=CC=N1 BSKHPKMHTQYZBB-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 moisture Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical compound CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- 230000002441 reversible effect Effects 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The utility model discloses a gas purification device and a glove box, comprising: an air inlet pipeline; an air outlet pipeline; an adsorption column; an oxygen adsorption material layer is arranged in the adsorption column; a circulating fan; a regeneration device. The oxygen adsorption material and the inert gas purging or vacuumizing physical mode are used, the reversibility of the combination of the oxygen adsorption material and oxygen molecules and the mechanism influenced by the oxygen pressure are utilized, so that the oxygen molecules adsorbed by the oxygen adsorption material are separated from an adsorption state, and the oxygen adsorption function of the oxygen adsorption material is recovered by utilizing the inert gas purging or vacuumizing device. According to actual needs, (1) a vacuumizing mode can be adopted; or (2) normal or low pressure inert gas purging; or (3) the inert gas is filled and vacuumized for a plurality of times; or (4) the 3 modes are used for auxiliary heating to realize the regeneration of the oxygen adsorption material. Overcomes the complex and potential safety hazard existing in the prior art that hydrogen is reduced and regenerated at about 200 ℃.
Description
Technical Field
The utility model relates to the technical field of gas purification systems and glove boxes, in particular to a gas purification device and a glove box.
Background
Glove boxes are currently relatively advanced closed systems that provide an inert atmosphere filled space that is isolated from air. Glove boxes are typically made up of two parts, a box, which is a working space, and a gas purification system, which is used to maintain the atmosphere within the box to meet working requirements. The atmosphere in the case contains impurities such as oxygen, moisture, and organic solvents. The organic solvent can be removed by adsorption materials such as activated carbon, and the molecular sieve and the adsorbent such as activated alumina can adsorb water, and materials containing active metals such as copper catalyst are used for removing oxygen.
A conventional glove box gas purification system contains two purification columns, which may also be referred to as adsorption columns (adsorption column 10 and adsorption column 4 as shown in fig. 5), the adsorption column 10 is typically filled with activated carbon, and the adsorption column 4 is typically filled with a molecular sieve and a copper catalyst. Under the action of a circulating fan, gas in the box body enters an adsorption column 10 of a gas circulating system, organic solvent is adsorbed by active carbon in the column, the gas then enters an adsorption column 4, moisture and oxygen in the gas are respectively removed by a molecular sieve and a copper catalyst, the gas returns to the box body through the circulating fan, after the gas passes through a purifying system, part of oxygen, moisture and organic solvent impurities are removed, the purity of inert gas is improved, the purifying process is continuously carried out, and the gas in the box body is continuously purified, so that the purity of the gas is always maintained within the working requirement range.
The principle of the copper catalyst for removing oxygen is copper (which may beThe other active metal, but usually copper), reacts chemically with oxygen to form oxides such as copper oxide (2Cu+O) 2 =2cuo). The purification performance of the glove box is an important index of the glove box, and the atmosphere in the glove box is required to be always maintained within a required range.
When the impurity removing capability of the materials in the purification column is consumed, the materials are required to be replaced or regenerated after the adsorption saturation, the molecular sieve and the activated carbon can be replaced or regenerated, the regeneration of the molecular sieve and the activated carbon is simpler, and the materials are only required to be heated, and simultaneously, the moisture and the organic solvent which are physically adsorbed can be desorbed from the adsorbent by ventilation or vacuumizing, so that the adsorption material can recover the capability of removing the water and the organic solvent. The copper on the copper catalyst is oxidized to copper oxide, and the regeneration is complicated, and a reducing gas such as hydrogen is required to reduce the copper oxide to metallic copper (cuo+h) at about 200 ℃ 2 →Cu+H 2 O), approximately 20 hours. When in regeneration, the adsorption column cannot be used, because the hydrogen is used in the process, a higher temperature is needed, and the adsorption efficiency of the traditional oxygen absorbing material is obviously reduced along with the increase of the regeneration times; the traditional purification columns are separated due to different regeneration conditions, and the columns for adsorbing oxygen and water and the columns for adsorbing organic solvents are separated, so that two sets of adsorption columns are always prepared simultaneously in order to meet the uninterrupted requirement of a client experiment during regeneration, and more space planning and cost are needed.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present utility model provides a gas purification apparatus and a glove box.
In order to achieve the above purpose, the utility model is realized by the following technical scheme:
a gas purification apparatus comprising:
an air inlet pipeline;
an air outlet pipeline;
the inlet of the adsorption column is connected with the outlet of the air inlet pipe, and the outlet of the adsorption column is connected with the air outlet pipe; the plurality of adsorption columns can form a serial, parallel or serial-parallel structure, and parallel branches are usually used as standby, so that the inside of the parallel adsorption columns is generally the same in filling materials.
Wherein at least one adsorption column is filled with oxygen adsorption material or comprehensive adsorption material;
the circulating fan is arranged on the air inlet pipeline or the air outlet pipeline and is used for driving gas to enter from the air inlet pipeline and flow through the adsorption column and then be discharged from the outlet of the air outlet pipeline;
the regenerating device comprises a vacuumizing device and/or an inert gas filling device which are communicated with an adsorption column filled with oxygen adsorption materials or comprehensive adsorption materials.
The utility model thoroughly changes the technology of regenerating by utilizing high temperature and hydrogen in the prior art, adopts a vacuumizing mode, and utilizes the mechanism that the combination of the oxygen adsorption material and oxygen molecules is influenced by air pressure to ensure that the oxygen molecules adsorbed by the oxygen adsorption material are separated from an adsorption state and are sucked away by a vacuumizing device, thereby realizing the oxygen adsorption function of the oxygen adsorption material. According to actual needs, the regeneration of the oxygen adsorption material or the comprehensive adsorption material can be realized by adopting a mode of vacuumizing for a plurality of times, or a mode of filling inert gas and vacuumizing for a plurality of times, or an auxiliary inert gas introducing or heating vacuumizing mode. Overcomes the complex and potential safety hazard existing in the prior art that hydrogen is reduced and regenerated at about 200 ℃.
Further, the regeneration device also comprises an adsorption column heating device for heating the oxygen adsorption material layer or the comprehensive adsorption material layer in the adsorption column.
Further, the heating device comprises a heating element arranged inside or outside the adsorption column.
Further, the heating element comprises one or more combinations of an electric heating element, a liquid medium or a gaseous medium heating line.
Further, the heating device also comprises a temperature control device, and the temperature T1 is controlled to be 30-150 ℃, preferably 50-100 ℃.
Further, the adsorption column is one, the inlet side of the adsorption column is provided with a third valve, the gas purification device is further provided with a bypass pipeline, an inlet of the bypass pipeline is connected to a pipeline between the bypass pipeline and the third valve, an outlet of the bypass pipeline is connected to an inlet end of the circulating fan, the circulating fan is arranged on a pipeline between the second valve and an outlet of the air outlet pipeline, and a fourth valve is arranged on the bypass pipeline.
Further, the pipeline of the vacuumizing device is connected to the pipeline between the third valve or the second valve and the adsorption column.
Further, the adsorption columns are two or more in parallel, the inlet side and the outlet side of each adsorption column are respectively provided with a valve, and the upper end and the lower end of each adsorption column filled with oxygen adsorption materials or the upper end and the lower end of each adsorption column filled with comprehensive adsorption materials are respectively connected with the inert gas filling device and the vacuumizing device through pipelines.
Further, the oxygen adsorption material in the oxygen adsorption material layer or the synthetic adsorption material layer is in a plurality of cylindrical, spherical particle structures or honeycomb columnar structures.
The utility model also discloses a glove box, which comprises a glove box body and the gas purifying device, and is used for purifying the gas atmosphere in the glove box body.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present utility model and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIGS. 1-4 are schematic illustrations of 4 different embodiments of the gas purification apparatus and glove box of the present utility model.
Fig. 5 is a schematic diagram of a prior art.
Reference numerals in the drawings represent respectively:
a glove box body 1; an air inlet pipeline 2; an air outlet pipeline 3; a second valve 31; adsorption columns 4 and 8; a circulating fan 5; a third valve 22; a bypass conduit 7; a fourth valve 71; vacuum line valves 61 and 62
A vacuum-pumping device 6; valves on two sides of the adsorption column 8 are respectively 81 and 82; a nitrogen valve 91; a second nitrogen valve 92; a nitrogen cylinder 9; an adsorption column 10; the adsorption column 10 has inlet and outlet valves 11 and 12.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present utility model more clear, the technical solutions of the embodiments of the present utility model will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present utility model. It will be apparent that the described embodiments are some, but not all, embodiments of the utility model. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The utility model is further described below with reference to examples.
A gas purification apparatus comprising:
an air inlet pipeline 2;
an air outlet pipeline 3, on which a second valve 31 is arranged;
the inlet of the adsorption column 4 is connected with the outlet of the air inlet pipe 1, and the outlet of the adsorption column 4 is connected with the air outlet pipe 3; an oxygen adsorption material layer is arranged in the adsorption column 4; or an active carbon layer, a molecular sieve layer and an oxygen adsorption material layer are arranged at the same time, or an integrated adsorption layer paved after mixing and granulating the active carbon material, the molecular sieve material and the oxygen adsorption material is arranged in the adsorption column 4; the plurality of adsorption columns can form a serial, parallel or serial-parallel structure, and parallel branches are usually used as standby, so that the inside of the parallel adsorption columns is generally the same in filling materials.
The circulating fan 5 is arranged on the air inlet pipeline 2 or the air outlet pipeline 3 and is used for driving gas to enter from the air inlet pipeline 2 and flow through the adsorption column 4 and then be discharged from the outlet of the air outlet pipeline 3; in general, as in the examples of fig. 1 and 2, the circulation fan 5 is disposed on the air outlet duct 3.
The regenerating device comprises a vacuumizing device 6 communicated with the adsorption column 4.
In the prior art, the high temperature of about 200 ℃ and the hydrogen are utilized for regeneration, the equipment is complex, and the use of the hydrogen has higher risk. The utility model thoroughly changes the technology of regenerating by using irreversible chemical adsorption deoxidizing material and high temperature and hydrogen in the prior art, but uses the physical mode of purging or vacuumizing by using reversible adsorption deoxidizing material and inert gas, and utilizes the reversibility of the combination of oxygen adsorption material and oxygen molecules and the mechanism influenced by the oxygen pressure to lead the oxygen molecules adsorbed by the oxygen adsorption material to be separated from the adsorption state, and utilizes the inert gas purging or vacuumizing device to realize the recovery of the oxygen adsorption function of the oxygen adsorption material or the comprehensive adsorption material. According to actual needs, (1) a vacuumizing mode can be adopted; or (2) normal or low pressure inert gas purging; or (3) filling inert gas for many times and vacuumizing, or (4) heating in an auxiliary way by the 3 modes, so as to realize the regeneration of the oxygen adsorption material. Overcomes the complex and potential safety hazard existing in the prior art that hydrogen is reduced and regenerated at about 200 ℃.
In some embodiments, to reduce the time spent for oxygen adsorbent regeneration, the regeneration device further comprises an adsorbent column heating device for heating the oxygen adsorbent material layer or the integrated adsorbent material layer within the adsorbent column 4. The oxygen adsorption material has the adsorption capacity to oxygen, which is mainly influenced by air pressure, the lower the air pressure of oxygen is, the weaker the oxygen adsorption capacity is, the oxygen is separated from an adsorption state and is sucked away by a vacuumizing device, and meanwhile, the higher the temperature is, the weaker the adsorption capacity is, so that the separation of oxygen can be accelerated through temperature adjustment, and the heating temperature is generally set between 50 ℃ and 100 ℃.
In practical applications, the heating means comprise a heating element arranged inside or outside the adsorption column.
The heating element may employ one or more combinations of electrical heating elements, liquid medium or gaseous medium heating lines.
In practical application, the heating device further comprises a temperature control device, wherein the temperature T1 is controlled to be 30-150 ℃, and the temperature range is preferably 50-100 ℃. The temperature can be conveniently controlled according to the requirement.
In the example of fig. 1, the number of the adsorption columns 4 is one, the third valve 22 is arranged at the inlet side of the adsorption column 4, the gas purifying device is further provided with a bypass pipeline 7, the inlet of the bypass pipeline 7 is connected to the air inlet pipeline 2 before the third valve 22, the outlet is connected to the inlet end of the circulating fan 5, the circulating fan 5 is arranged on the pipeline between the second valve 31 and the outlet of the air outlet pipeline 3, and the bypass pipeline 7 is provided with a fourth valve 71. The bypass pipeline 7 is arranged because the circulating fan 5 can not be stopped when certain glove boxes or other devices using other purifying devices are operated, so that when the adsorption column 4 is saturated, the operation can only be stopped, the regenerating device is utilized to complete the regeneration of the oxygen adsorption material in the adsorption column 4, and then the device is restarted to operate, so that the circulating fan and the device are not stopped when the adsorption column 4 is regenerated, the bypass pipeline 7 and the fourth valve 71 are arranged, the fourth valve 71 is closed when the bypass pipeline 7 is in normal operation, the bypass pipeline 7 is not in operation, the fourth valve 71 is firstly opened, then the second valve 31 and the third valve 22 are closed when the oxygen adsorption material is required to be regenerated, and at the moment, the circulating fan 5 can continuously circulate the gas in the device through the bypass pipeline 7 without stopping. Then, a vacuum pipeline valve 61 on the vacuumizing pipeline is opened, the vacuumizing equipment 6 is opened, the adsorption column 4 is vacuumized, and the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is realized.
In some embodiments, the bypass line 7 and the fourth valve 71 are not necessary, and in the gas purification device provided with the bypass line 7, one or more adsorption columns are generally further provided on the air inlet pipeline 2 before the third valve 22, so that the adsorption column 4 is cut off by the bypass line 7 when the regeneration operation of the adsorption column 4 is performed, and the rest of the adsorption columns can continue to operate.
The pipeline of the vacuumizing device 6 is connected to the pipeline between the third valve 22 or the second valve 31 and the adsorption column 4. In the example of fig. 1, the line of the evacuation device 6 is connected to the line between the second valve 31 and the adsorption column 4.
In some embodiments, an inert gas filling device, such as a high purity nitrogen filling device, including piping and nitrogen valve 91, may also be connected between the third valve 22 and the adsorption column 4. When the vacuum regeneration is performed, the second valve 31 and the third valve 22 are closed, the vacuum pipeline valve 61 is opened to perform vacuum, the nitrogen valve 91 is opened, and the high-purity nitrogen is filled into the adsorption column 4 by the nitrogen tank or the nitrogen steel bottle 9, and the process is repeated for several times until the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is realized. Generally, the evacuation device 6 is connected below the oxygen adsorbing material layer, and the inert gas filling device is connected above the oxygen adsorbing material layer. For example, a vacuum 6 is connected to the lower part of the column 4, and an inert gas filling device is connected to the upper end cap of the column. In this way, the inert gas injected by the inert gas filling device passes through the oxygen adsorption material from top to bottom, so as to purge the oxygen adsorption material and promote oxygen to be separated from an adsorption state. The vacuumizing device vacuumizes the lower part of the oxygen adsorption material, so that the purging effect can be enhanced, and meanwhile, the oxygen is promoted to be pumped away from the adsorption state due to the reduction of the oxygen pressure. The oxygen pressure is 1 atmosphere, for example, the mixed gas pressure in the adsorption column, and when the oxygen concentration is 1%, the corresponding oxygen pressure is 1% unit atmosphere, so that the oxygen pressure represents a dual index of the oxygen concentration and the air pressure.
The pipeline of the vacuumizing device 6 is generally only connected to the tank body at the outlet side of the adsorption column or the outlet pipeline.
The inert gas filling device is generally only required to be communicated with a tank body at one side of the inlet of the adsorption column or connected to a pipeline at one side of the inlet of the adsorption column.
In other embodiments, the number of the adsorption columns is two or more in parallel, as shown in fig. 2, two adsorption columns (4 and 8 respectively) are arranged, the inlet side and the outlet side of each adsorption column are respectively provided with a valve, in the example of fig. 2, the valves on two sides of the adsorption column 4 are respectively 22 and 31, the valves on two sides of the adsorption column 8 are respectively 81 and 82, and a vacuumizing pipeline is arranged on a pipeline between the outlet side and the outlet side valve of each adsorption column, and the vacuumizing pipeline is connected with a vacuumizing device through one valve. In the example of fig. 2, the adsorption column 4 and the adsorption column 8 are connected to a vacuum device through a vacuum line and valves 61 and 62 on the corresponding lines, respectively. In the example of fig. 2, two columns may be used, one for operation and one for standby operation, with the standby column being activated when regeneration is required. Two or more adsorption columns can also work simultaneously, but when regeneration operation is carried out, only one by one or part of adsorption columns are used for regeneration operation, and the rest adsorption columns continue to work until all adsorption columns complete regeneration operation in turn.
In some embodiments, the inert gas filling device adopts a high-purity nitrogen filling device, which comprises a pipeline, a nitrogen valve 91 and a second nitrogen valve 92, wherein the nitrogen valve 91 and a corresponding pipeline are connected between the third valve 22 and the adsorption column 4, and the second nitrogen valve 92 and the pipeline thereof are connected between the valve 81 and the adsorption column 8. When the adsorption column 4 is vacuumized and regenerated, the second valve 31 and the third valve 22 are closed, the vacuum pipeline valve 61 is opened to vacuumize, the nitrogen valve 91 is opened, and high-purity nitrogen is filled into the adsorption column 4 by the nitrogen tank or the nitrogen steel cylinder 9 for several times, so that the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is realized. When the adsorption column 8 is vacuumized and regenerated, the valve 81 and the valve 82 are closed, the vacuum pipeline valve 62 is opened to vacuumize, the second nitrogen valve 92 is opened, and high-purity nitrogen is filled into the adsorption column 8 by the nitrogen tank or the nitrogen steel cylinder 9 and is repeated for several times until the regeneration of the oxygen adsorption capacity of the oxygen adsorption material is realized.
In some embodiments, as shown in fig. 3, an adsorption column 10 and inlet valves 11 and 12 of the adsorption column 10 are further disposed before the adsorption column 4, a bypass valve 72 of the adsorption column 10 is connected across the outer sides of the inlet valves 11 and 12, and the adsorption column 10 is additionally provided with a moisture adsorption material, such as a molecular sieve material, or one or more layers of activated carbon for adsorbing organic components, so that the adsorption column 4 can be fully filled with a single oxygen adsorption material, specifically for adsorbing oxygen. Of course, the inside of the adsorption column 4 can be a multifunctional adsorption material mixed with molecular sieve and active carbon. The regeneration of the activated carbon and the molecular sieve in the adsorption column 10 requires the use of a high-temperature regeneration device, and a heating device may be used in the adsorption column 10. The bypass line 7- stage bypass valves 71 and 72 provided in fig. 3 can cut the adsorption column 10 or the adsorption column 4 by opening and closing one of the two bypass valves, and the cut adsorption column can perform a regeneration operation. The adsorption columns 10 and 4 can thus be subjected to alternating regeneration operations by means of the bypass line.
Similarly, as shown in fig. 4, in the system with the spare adsorption columns of the adsorption column 4 and the adsorption column 8, the adsorption column 10 may be added at the front end, and the internal materials and principles thereof are the same as those of the example of fig. 3, and will not be described again.
Further, the adsorption material in the oxygen adsorption material layer or the comprehensive adsorption material layer is in a plurality of cylindrical particle structures. Of course, the structure of the particles is not limited to a cylindrical particle structure, and the particles can be spherical, hollow beads with holes, columns with honeycomb holes or other cube structures, the particles are piled up in an adsorption column to form an oxygen adsorption material layer or an integrated adsorption material layer, and gaps among the particles form a passage through which gas flows.
The oxygen adsorption material or the comprehensive adsorption material adopted by the utility model is prepared by the applicant of the utility model, and the preparation method of the oxygen adsorption material or the comprehensive adsorption material is original by the applicant of the utility model, and the preparation method is as follows:
step one, firstly preparing a ligand material:
connecting a 3L reaction container with a reflux condensing device, a constant-pressure dropping device, a temperature control device and a heating stirring device, vacuumizing and replacing, then filling inert gas, adding 2mol of 2.4-pentanedione, 3mol of acetic anhydride and 2.4mol of ethyl acetoacetate into the reaction container, reacting under the protection of the inert gas at the stirring speed of 300rpm, controlling the temperature of the mixed solution at 90 ℃, and after the mixed reaction solution is reacted and reflowed for 2 hours at a temperature control point, closing heating, and cooling to room temperature under the protection of the inert gas;
connecting the reaction container with a reduced pressure distillation device, checking the air tightness of the system of the device, starting a condensation stirring device under the condition of ensuring good air tightness, slowly connecting vacuum into the system of the device at room temperature at the stirring speed of 300rpm, adjusting the vacuum degree to 30KPa, controlling the boiling degree of the mixed liquid through the adjustment of the vacuum degree, gradually extracting byproducts in the mixture after the liquid drops are not dripped, improving the vacuum degree to 15KPa, slowly raising the temperature of the solution to 60 ℃, collecting the byproducts in the byproduct receiving container until no liquid drops drip, and recovering the system of the device to normal pressure;
changing the byproduct receiving container into a target intermediate product receiving container, adjusting the vacuum degree to 10KPa, gradually heating the reaction mixed solution to 100 ℃, starting boiling the solution, dripping liquid drops in the target intermediate product receiving container, finally heating to 115 ℃ by controlling the temperature of the solution, collecting the target intermediate product, and weighing, wherein the yield is 73%;
the target intermediate product reacts with ethylenediamine and methanol under the stirring condition, and the ratio of reactants is 2:1: and 6, filtering and drying after the reaction to obtain a target product, namely the oxygen absorbing material ligand, with the yield of 90%.
Step two, preparing an oxygen adsorption material:
preparation of raw materials: cobalt acetate, the ligand prepared in the first step, isopropanol, potassium hydroxide and picoline;
step1: to a 250mL beaker, 0.1mol of cobalt acetate and 0.1mol of ligand were added, isopropyl alcohol was added, the reagent concentration was controlled at 4mol.L-1 of cobalt acetate and ligand, stirring was started under heating (control temperature was 50 to 60 ℃ C.), and stirring rate was set at 400R/min, to obtain a mixed solution 1. In addition, 0.1mol of potassium hydroxide and isopropanol reagent are added into a 250mL conical flask, the concentration is controlled to be 4mol.L-1, and the mixture is heated and stirred at 60 ℃ until the solid is completely dissolved, so that a mixed solution 2 is obtained. Under the condition of heating and stirring the mixed solution 1, the mixed solution 2 is added into the mixed solution 1, and the addition is completed within 30 minutes. After holding the temperature for 4 hours, the reaction was stopped. The reaction solution was suction-filtered to obtain a reddish brown solid product COL in 95% yield.
Step2: adding 0.15mol of COL, 0.12mol of potassium hydroxide, 0.14mol of picoline and solvent methyl isopropyl alcohol into a 250mlL beaker, controlling the concentration of the reagent to be 4mol of potassium hydroxide, starting the experiment under the condition of heating and stirring, setting the stirring rate to 300R/min, and slowly heating to 75-85 ℃. After holding the temperature for 6 hours, the reaction was stopped.
And (3) treating a reaction solution: the reaction solution was filtered by a vacuum pump, and the obtained product was dried in 97% yield. The product was used as an oxygen absorbing material, and the oxygen absorption rate was 6.02%. The oxygen absorption rate refers to the percentage of oxygen absorption mass to oxygen absorption material mass.
The target product is subjected to a cyclic oxygen absorption test, and the method adopts continuous circulation modes such as oxygen blowing, nitrogen blowing, oxygen blowing again, nitrogen blowing again and the like, and is subjected to continuous oxygen absorption analysis for 6 times, and after the nitrogen blowing, the oxygen absorption material can be desorbed back to the original state, so that oxygen is absorbed circularly. The oxygen absorbing material can continuously absorb oxygen in a circulating way by means of the gas purging mode, and after the oxygen absorbing material is circulated for a plurality of times, the oxygen absorbing rate is 6%, and the oxygen absorbing rate is kept unchanged. Proved by the utility model, the oxygen absorbing material has high oxygen absorbing rate, can be continuously recycled, and has convenient and quick operation, energy conservation and environmental protection.
The utility model also discloses a glove box, which comprises a glove box body 1 as shown in fig. 1 and 2, and the gas purifying device for purifying the gas atmosphere in the glove box body.
For example, as shown in fig. 1, the glove box body 1 is a single-station glove box body having a length of 1200mm, a depth of 750mm, and a height of 900mm.
One or two adsorption columns 4 are of an ID of 200mm and a height of 200mm, a heating pipe is arranged in each adsorption column 4, two KF40 flanges are arranged above each column and are connected with two KF40 angle valves, one is a third valve 22 for circulating air inlet, and the other is a second valve 31 for circulating air outlet. In addition, the adsorption column 4 is also provided with an air supplementing pipeline and an air supplementing valve. The column was packed with 6kg of molecular sieve and 800 g of the novel adsorbent material.
In the initial operation, air is injected into the glove box, the fourth valve 71 and the circulating fan are opened, and the oxygen concentration is stable.
The second valve 31 and the third valve 22 were then opened, the fourth valve 71 was closed, and the cycle was continued for 20 minutes, with the oxygen concentration dropping from 1030PPM to 218PPM.
The fourth valve 71 is opened again, the second valve 31 and the third valve 22 are closed, the adsorption column 4 is heated to about 70 ℃, and the air (generally pure nitrogen) is supplied into the adsorption column 4 after vacuum pumping is performed for 60 minutes.
The second valve 31 and the third valve 22 were opened, the fourth valve 71 was closed, and the cycle was continued for 300 minutes, with the oxygen concentration falling from 218PPM to 8PPM.
The fourth valve 71 is opened again, the second valve 31 and the third valve 22 are closed, the adsorption column 4 is heated to about 70 ℃, and the air (generally pure nitrogen) is supplied into the adsorption column 4 after vacuum pumping is performed for 60 minutes.
The second valve 31 and the third valve 22 are opened, the fourth valve 71 is closed, and the cycle is continued for 200 minutes, and the oxygen concentration is reduced from 8PPM to below 1 PPM. After meeting the atmosphere requirement in the glove box, the glove box can start to work. When the oxygen on the oxygen adsorbent in the adsorption column 4 is saturated, it is necessary to perform the operation of regenerating the oxygen adsorption capacity of the oxygen adsorbent as described above.
The above embodiments are only for illustrating the technical solution of the present utility model, and are not limiting; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present utility model.
Claims (11)
1. A gas purification apparatus, comprising:
an air inlet pipeline;
an air outlet pipeline;
the inlet of the adsorption column is connected with the outlet of the air inlet pipe, and the outlet of the adsorption column is connected with the air outlet pipe;
wherein at least one adsorption column is filled with oxygen adsorption material or comprehensive adsorption material;
the circulating fan is arranged on the air inlet pipeline or the air outlet pipeline and is used for driving gas to enter from the air inlet pipeline and flow through the adsorption column and then be discharged from the outlet of the air outlet pipeline;
the regenerating device comprises a vacuumizing device and/or an inert gas filling device which are communicated with an adsorption column filled with oxygen adsorption materials or comprehensive adsorption materials.
2. The gas purification apparatus according to claim 1, wherein the regeneration apparatus further comprises an adsorption column heating means for heating the oxygen adsorption material layer or the integrated adsorption material layer in the adsorption column.
3. The gas purification device according to claim 2, wherein the heating means comprises a heating element arranged inside or outside the adsorption column.
4. A gas purification apparatus according to claim 3, wherein the heating element comprises one or a combination of an electric heating element, a liquid medium or a gaseous medium heating circuit.
5. The gas purification device according to claim 2, wherein the heating device further comprises a temperature control device, and the temperature T1 is controlled to be 30-150 ℃.
6. The gas purification device according to claim 5, wherein the adsorption column is one, a third valve is arranged at the inlet side of the adsorption column, a bypass pipeline is further arranged on the gas purification device, an inlet of the bypass pipeline is connected to a pipeline between the bypass pipeline and the third valve, an outlet of the bypass pipeline is connected to an inlet end of a circulating fan, the circulating fan is arranged on a pipeline between the second valve and an outlet of the air outlet pipeline, and a fourth valve is arranged on the bypass pipeline.
7. The gas purification apparatus according to claim 6, wherein the line of the evacuation apparatus is connected to a line between the third valve or the second valve and the adsorption column.
8. The gas purification device according to claim 5, wherein the number of the adsorption columns is two or more in parallel, the inlet side and the outlet side of each adsorption column are respectively provided with a valve, and the upper end and the lower end of each adsorption column provided with the oxygen adsorption material or the upper end and the lower end of the adsorption column provided with the comprehensive adsorption material are respectively connected with the inert gas filling device and the vacuumizing device through pipelines.
9. The gas purification apparatus according to claim 2, wherein the heating means further comprises temperature control means, and the temperature T1 is controlled to 50-100 ℃.
10. The gas purification apparatus according to any one of claims 1 to 9, wherein the oxygen adsorbing material in the oxygen adsorbing material layer or the integrated adsorption layer has a plurality of columnar structures of cylindrical, spherical, or honeycomb-like columnar structures.
11. A glove box comprising a glove box body, characterized by further comprising the gas purification apparatus according to any one of claims 1 to 10.
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| CN202223513797.4U CN219290992U (en) | 2022-12-28 | 2022-12-28 | Gas purification device and glove box |
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| CN202223513797.4U CN219290992U (en) | 2022-12-28 | 2022-12-28 | Gas purification device and glove box |
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